CN112316954A - Preparation of In having a hollow dodecahedron shape2O3-In2S3Method for preparing composite photocatalyst - Google Patents
Preparation of In having a hollow dodecahedron shape2O3-In2S3Method for preparing composite photocatalyst Download PDFInfo
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- CN112316954A CN112316954A CN202011204278.2A CN202011204278A CN112316954A CN 112316954 A CN112316954 A CN 112316954A CN 202011204278 A CN202011204278 A CN 202011204278A CN 112316954 A CN112316954 A CN 112316954A
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- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims description 5
- 239000002243 precursor Substances 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000013267 rho-ZMOF Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims abstract description 9
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- HYZJCKYKOHLVJF-UHFFFAOYSA-N 1H-benzimidazole Chemical compound C1=CC=C2NC=NC2=C1 HYZJCKYKOHLVJF-UHFFFAOYSA-N 0.000 claims abstract description 4
- ZEVWQFWTGHFIDH-UHFFFAOYSA-N 1h-imidazole-4,5-dicarboxylic acid Chemical compound OC(=O)C=1N=CNC=1C(O)=O ZEVWQFWTGHFIDH-UHFFFAOYSA-N 0.000 claims abstract description 4
- ZYYDOSLSINDXIQ-UHFFFAOYSA-N O.O.O.O.[In+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O Chemical compound O.O.O.O.[In+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O ZYYDOSLSINDXIQ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 4
- 238000001354 calcination Methods 0.000 claims abstract description 4
- 238000013329 compounding Methods 0.000 claims abstract 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 230000035484 reaction time Effects 0.000 claims description 4
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 abstract description 9
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 238000004729 solvothermal method Methods 0.000 abstract description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 15
- 238000000634 powder X-ray diffraction Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- WGQKYBSKWIADBV-UHFFFAOYSA-N benzylamine Chemical compound NCC1=CC=CC=C1 WGQKYBSKWIADBV-UHFFFAOYSA-N 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- NQTSTBMCCAVWOS-UHFFFAOYSA-N 1-dimethoxyphosphoryl-3-phenoxypropan-2-one Chemical compound COP(=O)(OC)CC(=O)COC1=CC=CC=C1 NQTSTBMCCAVWOS-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000000101 transmission high energy electron diffraction Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 238000002524 electron diffraction data Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/20—Sulfiding
Abstract
The invention provides a method for preparing In with a hollow dodecahedron shape2O3‑In2S3A method of compounding a photocatalyst, comprising: dissolving indium nitrate tetrahydrate, 4, 5-imidazole dicarboxylic acid and benzimidazole In an organic solvent, transferring the solution into a flask, heating for reaction for a period of time, centrifugally collecting a product after the reaction is finished, cleaning and drying to obtain an In-rho-ZMOFs precursor with a dodecahedron shape; dissolving In-rho-ZMOFs precursor and thioacetamide In a methanol solution to obtain a mixed solution, transferring the mixed solution into a reaction kettle, heating for reaction for a period of time, and after the reaction is finished, centrifuging and collecting the productThe mixture is washed and dried to obtain dodecahedron shaped MOF @ In2S3(ii) a A dodecahedral form of MOF @ In2S3Calcining In argon atmosphere for a period of time to obtain hollow dodecahedron-shaped In2O3‑In2S3A composite photocatalyst is provided. The invention takes thioacetamide as a vulcanizing agent, and the photocatalyst In is prepared by a solvothermal method2O3‑In2S3Purer In2O3And pure In2S3Has higher photocatalytic activity.
Description
Technical Field
The invention relates to a photocatalytic material, In particular to an In with a hollow dodecahedron shape2O3-In2S3A composite photocatalyst and a preparation method thereof.
Background
In2O3As an important n-type semiconductor oxide, it has a forbidden band width of 2.8eV, excellent stability and appropriate band potential, and in addition, it has good thermal stability and strong fluorescence signal in the visible and ultraviolet regions, and has been widely studied in the field of visible light photocatalysis. In analogously to other monocomponent inorganic semiconductor photocatalysts2O3The prepared material has low conductivity, and under the condition of illumination, the defects that secondary recombination is easy to occur between photogenerated electrons and holes of the material and the like seriously affect the application of the material in photocatalysis. And metal sulfides such as In2S3Has a forbidden band width of about 2.07eV and has a good photoresponse range in a visible light region. In is mixed with2S3And In2O3After recombination, the visible absorption range of the material can be improved, and the separation efficiency of electrons and holes can also be improved. In addition, the hollow structure of the material can improve the utilization rate of incident light and the diffusion efficiency of reaction molecules, expose more active sites for catalytic reaction, improve the usability of the inner surface of the material and further have good photocatalytic property. However, an In having a hollow dodecahedron shape was designed and prepared2O3-In2S3Composite photocatalysts remain a significant challenge.
Disclosure of Invention
The invention selects thioacetamide as a vulcanizing agent, and then further vulcanizes the In-rho-ZMOFs precursor by a solvothermal method to prepare the hollow dodecahedral In2O3-In2S3Composite nanomaterial and photocatalyst In prepared therefrom2O3-In2S3Purer In2O3And pure In2S3Has higher photocatalytic activity.
Specifically, the present invention provides an In having a hollow dodecahedron form2O3-In2S3The preparation method of the composite photocatalyst comprises the following steps:
s1: dissolving indium nitrate tetrahydrate, 4, 5-imidazole dicarboxylic acid and benzimidazole In an organic solvent, transferring the solution into a flask, heating for reaction for a period of time, centrifugally collecting a product after the reaction is finished, cleaning and drying to obtain an In-rho-ZMOFs precursor with a dodecahedron shape;
s2: dissolving In-rho-ZMOFs precursor and thioacetamide In a methanol solution to obtain a mixed solution, transferring the mixed solution into a reaction kettle, heating for reaction for a period of time, centrifugally collecting a product after the reaction is finished, cleaning and drying to obtain the dodecahedron shaped MOF @ In2S3；
S3: a dodecahedral form of MOF @ In2S3Calcining In argon atmosphere for a period of time to obtain hollow dodecahedron-shaped In2O3-In2S3A composite photocatalyst is provided.
The organic solvent in the step S1 is N, N-dimethylformamide.
In the step S1, the heating temperature is 120 ℃, and the reaction time is 4 h.
In the step S2, the mass ratio of the In-rho-ZMOFs precursor to thioacetamide is 5: 2.
The heating temperature in said step S2 was 150 ℃ and the reaction time was 4 h.
The invention also provides the In with the hollow dodecahedron shape prepared by the method2O3-In2S3A composite nanomaterial.
Drawings
FIG. 1a is a Scanning Electron Micrograph (SEM) of an In-rho-ZMFs precursor alone prepared In an example of the present invention and FIGS. 1(b-f) are Elemental Distributions (EDX) of the In-rho-ZMFs precursor, FIG. 1g is a Scanning Electron Micrograph (SEM) of an In-rho-ZMFs precursor prepared In an example of the present invention, and FIG. 1h is an X-ray powder diffraction (XRD) of an In-rho-ZMFs precursor prepared In an example of the present invention;
FIG. 2a is a MOF @ In prepared according to an embodiment of the present invention2S3X-ray powder diffractogram (XRD), FIG. 2b is MOF @ In2S3Scanning Electron Microscopy (SEM), FIG. 2c is MOF @ In alone2S3Scanning Electron Micrographs (SEM) and FIG. 2(d-h) are the corresponding Elemental Distributions (EDX);
FIG. 3a shows In prepared by an example of the present invention2O3-In2S3Scanning Electron Micrograph (SEM) of the composite Structure and FIG. 3b is In2O3-In2S3Composite X-ray powder diffractogram (XRD);
in FIG. 4, a is In prepared In the examples of the present invention2O3-In2S3TEM image of the composite, b is a partial magnified view of the corresponding electron diffraction pattern (SAED). c is In prepared In the examples of the invention2O3-In2S3HRTEM images of the composite;
FIG. 5 shows In prepared by an example of the present invention2O3-In2S3Composite material, In2O3And In2S3Solid ultraviolet light of (1);
FIG. 6 shows In under simulated sunlight irradiation2O3-In2S3，In2O3，In2S3The coupling reaction of benzylamine is shown in the figure.
The specific implementation mode is as follows:
the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Examples
The first step is as follows: synthesis of In-rho-ZMOFs precursors
0.015g of indium nitrate tetrahydrate, 0.021g of 4, 5-imidazole dicarboxylic acid and 0.1g of benzimidazole were dissolved in 6ml of N, N-dimethylformamide, and the solution was transferred to a 25ml round-bottom flask and heated to 120 ℃ for 4 hours. And after the reaction is finished, collecting a product through centrifugation, washing the product for several times by using absolute ethyl alcohol, and drying the product In a drying box to obtain the dodecahedron-shaped In-rho-ZMOFs precursor.
The second step is that: synthesis of MOF @ In2S3
Taking 50mg of In-rho-ZMOFs precursor and 20mg of thioacetamide, dissolving the precursors and 20mg of thioacetamide In 9mL of methanol solution, transferring the mixed solution into a 25mL of polytetrafluoroethylene autoclave, and heating to 150 ℃ for 4 hours. After the reaction is finished, collecting the product by centrifugation, washing the product for a plurality of times by using absolute ethyl alcohol and deionized water, and placing the product In a drying box for drying to obtain the MOF @ In2S3A composite material.
The third step: synthesis of In2O3-In2S3Composite material
Taking MOF @ In2S3Calcining the mixture for 2 hours at 500 ℃ In an argon atmosphere to obtain In2O3-In2S3A composite material. FIG. 1a is an X-ray powder diffraction (XRD) pattern of an In-rho-ZMFs precursor alone prepared In an example of the present invention and FIG. 1b is an In-rho-ZMFs precursor Scanning Electron Micrograph (SEM), FIG. 1C is an SEM pattern of an In-rho-ZMFs precursor alone prepared In an example of the present invention and FIGS. 1(d-h) are corresponding Elemental Distributions (EDXs). FIG. 2a is a MOF @ In prepared according to an embodiment of the present invention2S3X-ray powder diffractogram (XRD), FIG. 2b is MOF @ In2S3Scanning Electron Microscopy (SEM), FIG. 2c is MOF @ In alone2S3Scanning Electron Micrographs (SEM) and FIG. 2(d-h) are the corresponding Element Distributions (EDX). FIG. 3a shows In prepared by an example of the present invention2O3-In2S3Scanning Electron Micrograph (SEM) of the composite Structure and FIG. 3b is In2O3-In2S3X-ray powder diffraction Pattern (XRD) of the composite Material, fig. 4a is In prepared by example of the present invention2O3-In2S3TEM image of the composite, FIG. 4b is the corresponding electron diffraction (SAED) sectionEnlargement. FIG. 4c shows In prepared by an embodiment of the present invention2O3-In2S3HRTEM images of composite materials. FIG. 5 shows In prepared by an example of the present invention2O3-In2S3Composite material, In2O3And In2S3Ultraviolet light of solids of (1). FIG. 6 shows In under simulated sunlight2O3-In2S3，In2O3，In2S3The results of the comparison of the benzyl amine catalysis show that the photocatalyst In can be seen from FIG. 62O3-In2S3Purer In2O3And pure In2S3Has higher photocatalytic activity.
Claims (6)
1. Preparation of In having a hollow dodecahedron shape2O3-In2S3The method for compounding the photocatalyst is characterized by comprising the following steps of:
s1: dissolving indium nitrate tetrahydrate, 4, 5-imidazole dicarboxylic acid and benzimidazole In an organic solvent, transferring the solution into a flask, heating for reaction for a period of time, centrifugally collecting a product after the reaction is finished, cleaning and drying to obtain an In-rho-ZMOFs precursor with a dodecahedron shape;
s2: dissolving In-rho-ZMOFs precursor and thioacetamide In a methanol solution to obtain a mixed solution, transferring the mixed solution into a reaction kettle, heating for reaction for a period of time, centrifugally collecting a product after the reaction is finished, cleaning and drying to obtain the dodecahedron shaped MOF @ In2S3；
S3: a dodecahedral form of MOF @ In2S3Calcining In argon atmosphere for a period of time to obtain hollow dodecahedron-shaped In2O3-In2S3A composite photocatalyst is provided.
2. The method of claim 1, wherein the organic solvent is N, N-dimethylformamide.
3. The method of claim 1, wherein in step S1, the heating temperature is 120 ℃ and the reaction time is 4 h.
4. The method of claim 1, wherein In the step S2, the mass ratio of the In-rho-ZMOFs precursor to thioacetamide is 5: 2.
5. The method of claim 1, wherein the heating temperature in step S2 is 150 ℃ and the reaction time is 4 h.
6. In having a hollow dodecahedron shape prepared by the method of any of the preceding claims2O3-In2S3A composite photocatalyst is provided.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114314641A (en) * | 2021-12-31 | 2022-04-12 | 汕头大学 | Preparation and application of ultrathin nanometer subunit assembled hollow indium sulfide nanorod |
| CN114965893A (en) * | 2022-05-24 | 2022-08-30 | 中国地质大学（武汉） | Preparation method of semiconductor metal oxide, gas sensor and preparation method thereof |
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| CN105664973A (en) * | 2016-02-26 | 2016-06-15 | 大连理工大学 | Three-dimensional flower-like In2S3/In2O3 composite microsphere photocatalytic material and preparation method thereof |
| CN109319826A (en) * | 2018-11-08 | 2019-02-12 | 江苏师范大学 | A kind of In with core-shell structure2O3The synthetic method of dodecahedron |
| CN109759082A (en) * | 2019-02-21 | 2019-05-17 | 黑龙江大学 | A kind of preparation method of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide |
| CN109999836A (en) * | 2019-04-28 | 2019-07-12 | 大连工业大学 | A kind of preparation of indium oxide/indium sulfide heterojunction semiconductor material and photochemical catalyst purposes and solar energy fixed nitrogen application |
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2020
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114314641A (en) * | 2021-12-31 | 2022-04-12 | 汕头大学 | Preparation and application of ultrathin nanometer subunit assembled hollow indium sulfide nanorod |
| CN114965893A (en) * | 2022-05-24 | 2022-08-30 | 中国地质大学（武汉） | Preparation method of semiconductor metal oxide, gas sensor and preparation method thereof |
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Application publication date: 20210205 |